A kind of refining method of acetylated impurity of vasopressin

A refining method, the technology of acetylation, which is applied in the field of refining acetylated impurities of vasopressin, can solve the problems of uneconomical, large amount of hazardous waste liquid, and high cost of waste liquid treatment, so as to reduce the amount of hazardous waste generated and optimize production The effect of craft

Active Publication Date: 2021-06-25
SPH NO 1 BIOCHEM & PHARMA CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The technical problem to be solved by the present invention is that in order to overcome the defects of high waste liquid treatment cost and uneconomical caused by the large amount of organic waste liquid produced in the refining process of vasopressin acetylated impurities in the prior art, and the large amount of hazardous waste liquid, A method for refining acetylated impurities of vasopressin is provided

Method used

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  • A kind of refining method of acetylated impurity of vasopressin
  • A kind of refining method of acetylated impurity of vasopressin
  • A kind of refining method of acetylated impurity of vasopressin

Examples

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preparation example Construction

[0052] In the following examples, the preparation method of the crude vasopressin acetylated impurity solution includes: (1) preparing the crude acetylated impurity of reduced vasopressin by solid-phase synthesis; (2) the acetylated impurity of reduced vasopressin The crude impurity product is dissolved and diluted to obtain a crude product solution of acetylated impurities of reduced vasopressin; (3) the crude product solution of acetylated impurities of reduced vasopressin is subjected to an oxidation process to obtain the crude product solution of acetylated impurities of vasopressin.

[0053] The solid-phase synthesis method includes the following steps: using Rink Amide MBHA resin as a starting material, using Fmoc-protected amino acids as monomers, using HOBt / DIC as a condensation agent, and sequentially connecting amino acids one by one; adding peptide cutting reagents to carry out Cut the peptide, add methyl tert-butyl ether for precipitation, and obtain the crude produ...

Embodiment 1

[0054] Example 1 Load&Lock4002 preparative column with inner diameter of 50mm

[0055] Using Load&Lock dynamic axial compression and static locking technology, the packing is as described ODS-AQ, pore size 10nm, particle size 10μm, packed to a column bed pressure of 1000psi, Varian chromatography packing system, 300g dry powder as described ODS-AQ super water-resistant filler, 600mL isopropanol is stirred and homogenized, poured into a Load&Lock4002 preparation column with an inner diameter of 50mm, the compression ratio is 1.5:1, and the carrier gas is N 2 , adjust the carrier gas pressure so that the oil pressure gauge pressure is 1500psi, and dynamically axially compress to a column bed height of 25cm, which is used as a preparative column for reverse-phase enrichment, reverse-phase salt conversion and reverse-phase purification schemes.

Embodiment 2

[0056] Example 2 Reverse-phase enrichment, reverse-phase salt conversion and reverse-phase purification of the crude product solution of vasopressin acetylation impurity

[0057] Instrument: Varian SD-1 high pressure liquid phase preparation system

[0058] Chromatographic column: the preparation column Load&Lock400250 * 250mm of embodiment 1, packing is ODS-AQ has a particle size of 10 μm and a pore size of 10 nm.

[0059] The structural formula of the acetylated impurity of vasopressin is The concentration of the crude acetylated impurity solution of reduced vasopressin is 1 mg / mL, and the solvent of the crude acetylated impurity solution of vasopressin is an aqueous solution containing trifluoroacetic acid and acetic acid.

[0060] Mobile phase A is 0.02% acetic acid / water solution by volume, mobile phase B is 0.02% acetic acid / acetonitrile by volume, and sample C1 is the crude product solution of acetylated impurities of vasopressin. The HPLC purity of the acetylated ...

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Abstract

The invention discloses a method for refining acetylated impurities of vasopressin. The method for refining the acetylated impurity of vasopressin comprises the following steps: the crude product solution of the acetylated impurity of vasopressin is sequentially subjected to reverse-phase enrichment, reverse-phase salt conversion, and reverse-phase purification by high-performance liquid phase chromatography; The packing of the high performance liquid reversed-phase chromatography is a super-water-resistant packing; the reverse-phase enrichment, reverse-phase salt conversion, and reverse-phase purification are all completed in a one-step reverse-phase elution process. The purification method of the vasopressin acetylation impurity of the present invention produces mostly waste water in the purification process, which can be reused after simple treatment at a sewage station, and is economical and environmentally friendly.

Description

technical field [0001] The invention relates to a method for refining acetylated impurities of vasopressin. Background technique [0002] Vasopressin is a synthetic polypeptide consisting of nine amino acid residues with a chemical structure of The theoretical molecular weight of vasopressin is 1084.24. Belongs to neurohypophyseal hormone, also known as vasopressin or vasopressin, it has two receptors V1 and V2. V1 is mainly distributed on the membrane of vascular smooth muscle cells, and acts through the receptor-G protein-second messenger pathway to constrict blood vessels and increase blood pressure. V2 is found in the epithelial cells of the distal tubule and collecting duct of the kidney, and physiological doses can promote the reabsorption of water by the distal tubule and collecting duct of the kidney, thereby exerting an antidiuretic effect. [0003] As far as a drug is concerned, a small amount of impurities contained in it is the most important cause of side ef...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07K7/16C07K1/20
Inventor 江锡铭丁金国黄臻辉
Owner SPH NO 1 BIOCHEM & PHARMA CO LTD
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